CN103487436A - Quantitative detection method of melamine chromaticity in raw milk and dairy products - Google Patents
Quantitative detection method of melamine chromaticity in raw milk and dairy products Download PDFInfo
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Abstract
The invention discloses a quantitative detection method of melamine chromaticity in raw milk and dairy products, belongs to a detection method of melamine in the raw milk and dairy products, and particularly relates to a detection method of melamine chromaticity. The method comprises three processes of sample pretreatment, detection of a sample solution to be detected, and judgment of melamine concentration of the sample solution to be detected, wherein quantitative treatment is adopted at the sample pretreatment stage; a color image sensor is adopted to image at the stage of judgment of the melamine concentration of the sample solution to be detected, so as to obtain RGB (red, green and blue) images; the concentration of the melamine is obtained by judging the mean value of each color in the RGB images. The method disclosed by the invention not only belongs to an objective judgment method, but also is accurate in detection result; the problem that different persons can obtain different detection results due to subjective judgment is effectively avoided; meanwhile, the process of judging the melamine content is an automatic judgment process, so that the detection speed is improved.
Description
Technical field
A kind of raw milk and melamine in dairy products colourity quantitative detecting method belong to the detection method of raw milk and melamine in dairy products, relate in particular to a kind of melamine chroma detection method.
Background technology
Melamine is a kind of broad-spectrum Organic Chemicals, and topmost purposes is as the raw material of producing melamine formaldehyde resin, can also be used as fire retardant, water reducer, formaldehyde detersive etc.
Because the protein content of food is mainly estimated by China by measuring nitrogen content, and the nitrogen content of melamine is about 66%, far away higher than the average nitrogen content 16% of protein, therefore, in order to pursue the raising of nitrogen content, some mixes melamine in food without good illegal retailer, makes the protein test content virtual height of food, thereby poor quality food is got by under false pretences.
Yet the food of this interpolation melamine does not only have really to increase the content of protein, its toxic and side effect can be given us on the contrary healthyly brings harm.Zoopery shows, takes in for a long time the infringement that melamine can cause reproduction, urinary system, causes bladder, kidney section calculus, and can further bring out carcinoma of urinary bladder.
2008, the event that the Sanlu baby milk powder adds melamine was broken out in China, and the cause that this event is exposed has been to eat the infant who adds melamine milk powder and has produced the kidney stone illness.Visible, melamine mixes the practice of dairy products and has directly challenged food security, and the health that is threatening us.Therefore, in order to stop in dairy products to add melamine, need the melamine detection method of a kind of raw milk and dairy products.
Existing raw milk and dairy products melamine detection method mainly contain high performance liquid chromatography, Liquid Chromatography-Tandem Mass Spectrometry, gas chromatography-tandem mass spectrometry etc.Although these methods can realize the accurate detection of melamine, it needs exact instrument and professional's operation, and consuming time longer, testing cost is higher, in most of the food enterprises and ordinary consumer, is difficult to popularize.
In order to address this problem, patent of invention: the chroma detection method of raw milk and melamine in dairy products and kit (application number: 200910190869.6), disclose a kind of melamine chroma detection method, by comparing with colorimetric card, directly obtained the content of melamine.The method favorable reproducibility, do not need to use any expensive instrument, and easy and simple to handle cost is low fast, is easy to as common testing staff and consumption grasp.
Yet this method also has its inevitable shortcoming, owing to adopting colorimetric card to compare, belong to the subjective judgement method, different people is inconsistent to the judged result of color, therefore easily causes testing result inconsistent, simultaneously, color category on colorimetric card is limited, therefore make testing result comparatively wide in range, be not suitable for accurate detection, in addition, the process of judgement is artificial process, still makes detection speed be subject to certain limitation.
Summary of the invention
In order to address the above problem, the present invention has designed a kind of raw milk and melamine in dairy products colourity quantitative detecting method, the method not only belongs to objective determination methods, the different people of effectively avoiding subjective judgement to cause obtains the problem of different testing results, and testing result is accurate, the process that simultaneously judges content of melamine is automatization judgement, has improved detection speed.
The object of the present invention is achieved like this:
A kind of raw milk and melamine in dairy products colourity quantitative detecting method comprise the following steps:
Step a: sample pre-treatments
Get raw milk or liquid dairy products, ratio according to 1:1 is mixed with distilled water, add hydrochloric acid solution, extremely caseic isoelectric point makes casein precipitation, centrifuging and taking supernatant, ratio according to supernatant and absolute ethyl alcohol 1:10 adds absolute ethyl alcohol again, make all the other protein denaturation precipitations, the centrifuging and taking supernatant, add hydrochloric acid solution, regulate pH value to 2.0, as testing sample solution;
Step b: testing sample solution detects
To solution colour, be the testing sample solution that adds step a to obtain in the coated gold size solution of red mercaptoacetic acid, being made the reaction density of the coated gold size of mercaptoacetic acid with distilled water diluting 0 ~ 10 is 3.8 * 10
-5mol/L, mix, under room temperature standing 5 minutes;
Step c: testing sample solution melamine concentration judgement
Testing sample solution after step b processes is contained in transparent glass vessels, utilized the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in judgement RGB image, obtain the concentration of melamine.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 8, and every kind of color can have 256 numerical value, and the combination of three kinds of colors can detect 16777216 kinds of results altogether.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 6, and every kind of color can have 64 numerical value, and the combination of three kinds of colors can detect 262144 kinds of results altogether.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 4, and every kind of color can have 16 numerical value, and the combination of three kinds of colors can detect 4096 kinds of results altogether.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 2, and every kind of color can have 4 numerical value, and the combination of three kinds of colors can detect 64 kinds of results altogether.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, the RGB image in described step c, be the image obtained after the color image sensor imaging.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, the RGB image in described step c, for choosing the image of zone line after the color image sensor imaging.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, the RGB image in described step c, for carrying out the image after denoising after the color image sensor imaging.
Described denoising adopts Butterworth or gauss low frequency filter to realize.
Due to raw milk of the present invention and melamine in dairy products colourity quantitative detecting method, in the sample pre-treatments stage, be all quantitative Treatment, therefore can effectively avoid testing result because operating different inaccurate problems; In the testing sample solution melamine concentration judgement stage, utilize the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in judgement RGB image, obtain the concentration of melamine, so the method not only belongs to objective determination methods, the different people of effectively avoiding subjective judgement to cause obtains the problem of different testing results, and testing result is accurate, judge that the process of content of melamine is automatization judgement simultaneously, improved detection speed.
The accompanying drawing explanation
Fig. 1 is raw milk of the present invention and melamine in dairy products colourity quantitative detecting method process flow diagram.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the invention is described in further detail.
Specific embodiment one
The raw milk of the present embodiment and melamine in dairy products colourity quantitative detecting method comprise the following steps:
Step a: sample pre-treatments
Get raw milk or liquid dairy products, ratio according to 1:1 is mixed with distilled water, add hydrochloric acid solution, extremely caseic isoelectric point makes casein precipitation, centrifuging and taking supernatant, ratio according to supernatant and absolute ethyl alcohol 1:10 adds absolute ethyl alcohol again, make all the other protein denaturation precipitations, the centrifuging and taking supernatant, add hydrochloric acid solution, regulate pH value to 2.0, as testing sample solution;
Step b: testing sample solution detects
To solution colour, be the testing sample solution that adds step a to obtain in the coated gold size solution of red mercaptoacetic acid, being made the reaction density of the coated gold size of mercaptoacetic acid with distilled water diluting 0 ~ 10 is 3.8 * 10
-5mol/L, mix, under room temperature standing 5 minutes;
Step c: testing sample solution melamine concentration judgement
Testing sample solution after step b processes is contained in transparent glass vessels, utilized the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in the resulting RGB image of direct judgement, obtain the concentration of melamine.
In described step c, the degree of depth of every kind of color of RGB image is 8, and every kind of color can have 256 numerical value, and the combination of three kinds of colors can detect 16777216 kinds of results altogether.Adopt the image of 8 bit depth to make change color very responsive, therefore can detect the subtle change of content of melamine, improve testing result precision and sensitivity.
Specific embodiment two
The raw milk of the present embodiment and melamine in dairy products colourity quantitative detecting method comprise the following steps:
Step a: sample pre-treatments
Get raw milk or liquid dairy products, ratio according to 1:1 is mixed with distilled water, add hydrochloric acid solution, extremely caseic isoelectric point makes casein precipitation, centrifuging and taking supernatant, ratio according to supernatant and absolute ethyl alcohol 1:10 adds absolute ethyl alcohol again, make all the other protein denaturation precipitations, the centrifuging and taking supernatant, add hydrochloric acid solution, regulate pH value to 2.0, as testing sample solution;
Step b: testing sample solution detects
To solution colour, be the testing sample solution that adds step a to obtain in the coated gold size solution of red mercaptoacetic acid, being made the reaction density of the coated gold size of mercaptoacetic acid with distilled water diluting 0 ~ 10 is 3.8 * 10
-5mol/L, mix, under room temperature standing 5 minutes;
Step c: testing sample solution melamine concentration judgement
Testing sample solution after step b processes is contained in transparent glass vessels, utilized the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in the resulting RGB image of direct judgement, obtain the concentration of melamine.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 4, and every kind of color can have 16 numerical value, and the combination of three kinds of colors can detect 4096 kinds of results altogether.Adopt the image of 4 bit depth to make change color more responsive, can detect content of melamine than subtle change, for to testing result accuracy requirement not include high occasion very applicable.
Specific embodiment three
The raw milk of the present embodiment and melamine in dairy products colourity quantitative detecting method comprise the following steps:
Step a: sample pre-treatments
Get raw milk or liquid dairy products, ratio according to 1:1 is mixed with distilled water, add hydrochloric acid solution, extremely caseic isoelectric point makes casein precipitation, centrifuging and taking supernatant, ratio according to supernatant and absolute ethyl alcohol 1:10 adds absolute ethyl alcohol again, make all the other protein denaturation precipitations, the centrifuging and taking supernatant, add hydrochloric acid solution, regulate pH value to 2.0, as testing sample solution;
Step b: testing sample solution detects
To solution colour, be the testing sample solution that adds step a to obtain in the coated gold size solution of red mercaptoacetic acid, being made the reaction density of the coated gold size of mercaptoacetic acid with distilled water diluting 0 ~ 10 is 3.8 * 10
-5mol/L, mix, under room temperature standing 5 minutes;
Step c: testing sample solution melamine concentration judgement
Testing sample solution after step b processes is contained in transparent glass vessels, utilized the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in the resulting RGB image of direct judgement, obtain the concentration of melamine.
Above-mentioned a kind of raw milk and melamine in dairy products colourity quantitative detecting method, in described step c, the degree of depth of every kind of color of RGB image is 2, and every kind of color can have 4 numerical value, and the combination of three kinds of colors can detect 64 kinds of results altogether.Adopt the image of 2 bit depth to make change color insensitive, can effectively avoid impact testing result brought due to the parasitic light in environment, there is stronger interference free performance.
Specific embodiment four
The different RGB images that are in described step c of the present embodiment and specific embodiment one, specific embodiment two and specific embodiment three, for choosing the image of zone line after the color image sensor imaging.Select the sensitiveest zone line, increase the measuring accuracy of testing result.
Specific embodiment five
The different RGB images that are in described step c of the present embodiment and front embodiment, for carrying out the image after denoising after the color image sensor imaging, described denoising adopts Butterworth LPF to realize.This mode can be avoided the impact of imaging process high-frequency noises on testing result.
Specific embodiment six
The different RGB images that are in described step c of the present embodiment and front embodiment, for carrying out the image after denoising after the color image sensor imaging, described denoising adopts gauss low frequency filter to realize.This mode can be avoided the impact of imaging process high-frequency noises on testing result.
Claims (9)
1. a raw milk and melamine in dairy products colourity quantitative detecting method is characterized in that comprising the following steps:
Step a: sample pre-treatments
Get raw milk or liquid dairy products, ratio according to 1:1 is mixed with distilled water, add hydrochloric acid solution, extremely caseic isoelectric point makes casein precipitation, centrifuging and taking supernatant, ratio according to supernatant and absolute ethyl alcohol 1:10 adds absolute ethyl alcohol again, make all the other protein denaturation precipitations, the centrifuging and taking supernatant, add hydrochloric acid solution, regulate pH value to 2.0, as testing sample solution;
Step b: testing sample solution detects
To solution colour, be the testing sample solution that adds step a to obtain in the coated gold size solution of red mercaptoacetic acid, being made the reaction density of the coated gold size of mercaptoacetic acid with distilled water diluting 0 ~ 10 is 3.8 * 10
-5mol/L, mix, under room temperature standing 5 minutes;
Step c: testing sample solution melamine concentration judgement
Testing sample solution after step b processes is contained in transparent glass vessels, utilized the color image sensor imaging, obtain the RGB image, by the mean values of every kind of color in judgement RGB image, obtain the concentration of melamine.
2. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, it is characterized in that in described step c, the degree of depth of every kind of color of RGB image is 8, every kind of color can have 256 numerical value, and the combination of three kinds of colors can detect 16777216 kinds of results altogether.
3. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, it is characterized in that in described step c, the degree of depth of every kind of color of RGB image is 6, every kind of color can have 64 numerical value, and the combination of three kinds of colors can detect 262144 kinds of results altogether.
4. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, it is characterized in that in described step c, the degree of depth of every kind of color of RGB image is 4, and every kind of color can have 16 numerical value, and the combination of three kinds of colors can detect 4096 kinds of results altogether.
5. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, it is characterized in that in described step c, the degree of depth of every kind of color of RGB image is 2, and every kind of color can have 4 numerical value, and the combination of three kinds of colors can detect 64 kinds of results altogether.
6. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, is characterized in that the RGB image in described step c, is the image obtained after the color image sensor imaging.
7. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, is characterized in that the RGB image in described step c, for choosing the image of zone line after the color image sensor imaging.
8. a kind of raw milk according to claim 1 and melamine in dairy products colourity quantitative detecting method, is characterized in that the RGB image in described step c, for carrying out the image after denoising after the color image sensor imaging.
9. a kind of raw milk according to claim 8 and melamine in dairy products colourity quantitative detecting method, is characterized in that described denoising adopts Butterworth or gauss low frequency filter to realize.
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CN105973886A (en) * | 2016-05-30 | 2016-09-28 | 田发益 | Method and device for determining concentration value based on visible light spectrum |
CN106441488A (en) * | 2016-10-19 | 2017-02-22 | 杨林 | Method for measuring operative bleeding amount and measuring card |
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CN101650314A (en) * | 2009-09-15 | 2010-02-17 | 中国人民解放军第三军医大学 | Chroma detection method of tripolycyanamide contained in raw milk and milk product and kit |
CN102435558A (en) * | 2011-09-13 | 2012-05-02 | 河海大学常州校区 | CO2 sensor based on test solution color measurement and detection method thereof |
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CN101650314A (en) * | 2009-09-15 | 2010-02-17 | 中国人民解放军第三军医大学 | Chroma detection method of tripolycyanamide contained in raw milk and milk product and kit |
CN102435558A (en) * | 2011-09-13 | 2012-05-02 | 河海大学常州校区 | CO2 sensor based on test solution color measurement and detection method thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105973886A (en) * | 2016-05-30 | 2016-09-28 | 田发益 | Method and device for determining concentration value based on visible light spectrum |
CN105973886B (en) * | 2016-05-30 | 2019-03-29 | 田发益 | A kind of method and device determining concentration value based on visible light |
CN106441488A (en) * | 2016-10-19 | 2017-02-22 | 杨林 | Method for measuring operative bleeding amount and measuring card |
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